FeClH(P(CH2CH2PMe2)3 | 189447-25-4

• 分子结构分类: 有机化合物 - 有机磷化合物 - 有机膦及其衍生物
• 英文名称: FeClH(P(CH2CH2PMe2)3
• 英文别名: chloro(hydrido)iron;tris(2-dimethylphosphanylethyl)phosphane
• CAS: 189447-25-4
• 化学式: C₁₂H₃₁ClFeP₄
• 分子量: 390.573
• InChiKey: LOJQZFBNADVRLP-UHFFFAOYSA-M

计算性质

• 辛醇/水分配系数(LogP)：
  None
• 重原子数：
  None
• 可旋转键数：
  None
• 环数：
  None
• sp3杂化的碳原子比例：
  None
• 拓扑面积：
  None
• 氢给体数：
  None
• 氢受体数：
  None

反应信息

• 作为反应物：
  描述：

  甲醇 、 FeClH(P(CH2CH2PMe2)3 以 甲醇 为溶剂， 生成 FeH(OMe)(tris[2-(dimethylphosphino)ethyl]phosphine)
  参考文献：
  名称：

  Field, Leslie D.; Messerle, Barbara A.; Smernik, Ronald J., Inorganic Chemistry, 1997, vol. 36, # 26, p. 5984 - 5990

  摘要：

  DOI：
• 作为产物：
  描述：

  FeCl2(tris[2-(dimethylphosphino)ethyl]phosphine) 、 lithium aluminium tetrahydride 以 四氢呋喃 为溶剂， 以78%的产率得到FeClH(P(CH2CH2PMe2)3
  参考文献：
  名称：

  Iron Complexes Containing the Tripodal Tetraphosphine Ligand P(CH₂CH₂PMe₂)₃

  摘要：

  The preparation and characterization of iron(II) complexes containing the tripodal tetraphosphine ligand tris[2-(dimethylphosphino)ethyl]phosphine, P(CH2CH2PMe2)(3) (PP3, 1), are reported. The complex FeCl2(PP3) (2) was formed by the reaction of PP3 with anhydrous iron(II) chloride. The complexes FeHCl(PP3) (3) and FeH2(PP3) (4) were formed by the reaction of 2 with Lithium aluminum hydride. Likewise, the complexes FeMeCl(PP3) (5) and FeMe2(PP3) (6) were formed by the reaction of 2 with methyllithium or dimethylmagnesium. Reaction of 2 with CO afforded a mixture of isomeric carbonyl chloride complexes [Fe(CO)Cl(PP3)](+) (7 and 8). Reaction of 2 with PPh3 afforded. [Fe(PPh3)Cl(PP3)](+) (9). The air-sensitive complexes 2-9 were characterized by multinuclear NMR spectroscopy, and 9 was characterized by X-ray crystallography. Crystals of 9 (BPh4 salt), C54H65BClFeP5, M971.09, arts monoclinic, space group P2(1)/c, a = 13.246(3) Angstrom, b = 30.314(2) Angstrom, c = 14.338(2) Angstrom, beta = 100.92(2)degrees, Z = 4; R = 0.058.

  DOI：

  10.1021/ic970030b

文献信息

• An iron(ii) dihydrogen hydrido complex containing the tripodal tetraphosphine ligand P(CH2CH2PMe2)3
  作者：Leslie D. Field、Hsiu L. Li、Barbara A. Messerle、Ronald J. Smernik、Peter Turner

  DOI：10.1039/b401954g

  日期：——

  complex FeH2(PP3) 3 with methanol or ethanol. The observation of H–D coupling in partially deuterated isotopomers of 1 and measurement of T1 relaxation times for the hydrido and dihydrogen resonances of 1 confirmed the presence of the η2-dihydrogen ligand. Complex 1 shows dynamic NMR behaviour in both the 31P and 1H NMR spectra with facile exchange between the protons in the η2-dihydrogen ligand and the

  二氢盐氢基络合物[FEH（H 2）（PP 3）] + 1 （PP 3 = P（CH 2 CH 2 PME 2）3 2）通过dihydrido的质子化复杂FEH形成2（PP 3） 3与甲醇或乙醇。H-d耦合在部分氘化同位素的观察1的和测量Ť 1弛豫时间的氢基和二氢共振1证实了η存在2 -dihydrogen配体。综合大楼1示出了在两个动态NMR行为31 P和1 1 H NMR谱与在η的质子之间容易交换2 -dihydrogen配体和η 1 -hydrido配体。的二氢配体1容易通过阴离子和中性配位体置换，得到相应的氢基配合物[FeHX（PP 3）] + （X = CO 11，X = PPH 3 12）或FeHX（PP 3）（X =氯13，X ＝ Br 14，X ＝ I 15，X ＝ N 3 16）。少量烷氧基氢化物FeH（OR）（PP3）在含有1的甲醇和乙醇溶液中观察到（R = Me 4 ;
• Butenynyl complexes of iron(II) containing the tripodal tetraphosphine ligand P(CH2CH2PMe2)3
  作者：Leslie D. Field、Barbara A. Messerle、Ronald J. Smernik、Trevor W. Hambley、Peter Turner

  DOI：10.1039/a902784j

  日期：——

  The preparation and characterisation of iron(II) η3-but-1-en-3-yn-2-yl complexes [Fe(η3-RCC–CCHR)L]+ [L = P(CH2CH2PMe2)3, R = Ph 1; R = But 2; R = p-HCCC6H4 3] is reported. The phenyl substituted butenynyl complex 1 was prepared by the reaction of FeCl2L 5, FeH(Cl)L 6 or [FeH(H2)L]+ 7 with phenylacetylene in alcohol solvent. The coordinated but-1-en-3-yn-2-yl fragment is bound as a σ-vinyl/π-acetylenic ligand. In solution, complex 1 exists as a pair of equilibrating isomers (1a and 1b) which differ in the anchoring mode of the butenynyl ligand i.e. depending on whether the π-bound acetylenic group is cis or trans to the apical phosphorus of L in the octahedral coordination sphere. Assignment of the relative stereochemistry of 1a and 1b was achieved by analysis of the 2D NOESY spectrum. Exchange peaks in the NOESY spectrum also provided information on the mechanism of exchange between 1a and 1b. The crystal structure of 1 showed the solid state structure to be that of the major solution state isomer 1a (π-bound acetylenic group is cis to the apical phosphorus of L). Complex 1 catalyses the stereospecific head-to-head dimerisation of phenylacetylene to Z-1,4-diphenylbut-1-en-3-yne.

  报告了铁（II）η3-丁-1-烯-3-炔-2-基配合物 [Fe(η3-RCC-CCHR)L]+ [L = P(CH2CH2PMe2)3, R = Ph 1; R = But 2; R = p-HCCC6H4 3] 的制备和表征。苯基取代的丁炔基配合物 1 是通过 FeCl2L 5、FeH(Cl)L 6 或 [FeH(H2)L]+ 7 与苯乙炔在醇溶剂中反应制备的。配位的丁-1-烯-3-炔-2-基片段作为σ-乙烯基/π-乙炔配体结合在一起。在溶液中，配合物 1 存在一对平衡异构体（1a 和 1b），它们在丁炔配体的锚定方式上有所不同，即取决于π结合的乙炔基与八面体配位层中 L 的顶端磷是顺式还是反式。通过分析二维 NOESY 光谱，可以确定 1a 和 1b 的相对立体化学结构。NOESY 光谱中的交换峰还提供了有关 1a 和 1b 交换机制的信息。1 的晶体结构显示其固态结构为主要溶液态异构体 1a（π-结合的乙炔基与 L 的顶端磷为顺式）。复合物 1 催化苯乙炔立体定向头对头二聚为 Z-1,4-二苯基丁-1-烯-3-炔。
• Mixed-Valence Dinitrogen-Bridged Fe(0)/Fe(II) Complex
  作者：Leslie D. Field、Ruth W. Guest、Peter Turner

  DOI：10.1021/ic101646p

  日期：2010.10.4

  The reactions of a dinitrogen-bridged Fe(II)/Fe(II) complex [(FeH(PP3))(2)(mu-N-2)](2+) (3) (PP3 = P(CH2CH2PMe2)(3)) with base were investigated usin N-15 labeling techniques to enhance characterization. In the presence of base, 3 is initially deprotonated to the Fe(II)/Fe(0) dinitrogen-bridged complex [(FeH(PP3))(kt-N-2)(Fe(PP3))]' (4) and then to the symmetrical Fe(0)/Fe(0) dinilrogen-bridged complex (Fe(PP3))(2)(u-N-2) (5). [(FeH(PP3))(j4-N2)(Fe(PP3))](+) (4) exhibits unusual long-range 31P-31P NMR coupling through the bridging dinitrogen ligand from the phosphines at the Fe(0) center and those at the Fe(II) center. Reaction of 4 with base under an atmosphere of argon resulted in the known dinitrogen Fe(0) complex Fe(N-2)(PP3) (6) and a solvent C H activation product. Complexes 3, 4, and 5 were fully characterized by multinuclear NMR spectroscopy, and complexes 3 and 4 by X-ray crystallography.